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Preparation method of micron monodisperse copolymerization microsphere

A monodisperse, micron-scale technology, used in the preparation of micron-scale monodisperse copolymer microspheres, can solve the problems of inability to meet, poor heat resistance, difficult to monodisperse uniform microspheres, etc., and achieve the effect of uniform size

Inactive Publication Date: 2007-03-14
YANTAI SHUODE NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the emulsion polymerization method can prepare microspheres with good dispersion, it can only prepare microspheres with a particle size of less than 0.5 μm; the polymer microspheres produced by the suspension polymerization method have a particle size of 100 μ to 1000 μm, and they are all polydisperse. ; Dispersion polymerization is a more effective method for preparing micron-scale monodisperse polymer microspheres. The one-step dispersion polymerization method of styrene is more researched. The particle size and monodispersity of the prepared microspheres are all very good. However, the heat resistance is poor, and the microspheres will melt immediately when they reach 150°C, which cannot meet the requirements of polymer conductive microspheres as an anisotropic conductive film; It is difficult to obtain uniform microspheres with good monodispersity by one-step dispersion polymerization of cross-linking agents such as ester (EGDMA)
Therefore, it is very difficult to prepare monodisperse micron-sized polymer microspheres with a particle size between 1 and 10 μm that meet the requirements for anisotropic conductive films by these methods.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0033] Add 15.0g of styrene, 0.15g of AIBN, 2.7g of PVP-K30, 0.5g of aerosol OT, 60.0g of ethanol, and 60.0g of ethylene glycol monomethyl ether into a 250mL four-necked reaction flask, which is equipped with a reflux device, stirring device, temperature measuring device, N 2 Protective device, heated in a water bath. N 2 Insert the inlet tube under the liquid phase, replace the air for 1h, and then add N 2 The inlet pipe is raised to the gas phase and continues to pass N 2 . Rapidly raise the temperature to 70°C, and polymerize for 24 hours at a stirring speed of 80 rpm. After the polymerization was completed, the reactant was settled by ultracentrifugation, the supernatant was discarded, and the microspheres in the lower layer were washed 5 times with ethanol. Pour the washed microspheres into a petri dish, and dry them in a vacuum oven at 60°C for 24 hours to obtain polystyrene microsphere seeds with an average diameter D of 1.5 μm.

example 2

[0035] Put 0.3g of PS seeds, 0.3g of CD, and 100g of 0.25% SLS aqueous solution into a beaker, and sonicate in an ultrasonic homogenizer for 10 minutes; after completion, transfer the solution to a four-necked reaction flask, and swell at 30°C for 10 hours, stirring at a speed of 200rpm.

[0036] 100g of an aqueous solution of St6g, DVB1g, EGDMA3g, and 0.25% SLS was sonicated in an ultrasonic homogenizer for 5min, transferred to a reaction bottle, and swelled at 30°C for 12h.

[0037] After the swelling is completed, add 40g of 5% PVP aqueous solution; add AIBN 0.1g; 2 After 1h, polymerize at 70°C for 16h.

[0038] After the polymerization was completed, it was washed repeatedly with water and ethanol, and dried in vacuum. The emulsion sample was settled by ultracentrifugation, the supernatant was discarded, and the microspheres in the lower layer were washed with ethanol, and this was repeated 5 times. Pour the washed microspheres into a petri dish, and dry them in a vacuu...

example 3

[0040] Put 0.3g of PS seeds, 0.3g of CD, and 100g of 0.25% SLS aqueous solution into a beaker, and sonicate in an ultrasonic homogenizer for 10 minutes; after completion, transfer the solution to a four-necked reaction flask, and swell at 30°C for 10 hours, stirring at a speed of 200rpm.

[0041] 100 g of an aqueous solution of St9g, DVB 0.5 g, EGDMA 0.5 g, and 0.25% SLS was sonicated in an ultrasonic homogenizer for 5 min, transferred to a reaction bottle, and swelled at 30° C. for 12 h.

[0042] After the swelling is completed, add 40g of 5% PVP aqueous solution; add AIBN 0.1g; 2 After 1h, polymerize at 70°C for 16h.

[0043]After the polymerization was completed, it was washed repeatedly with water and ethanol, and dried in vacuum. The emulsion sample was settled by ultracentrifugation, the supernatant was discarded, and the microspheres in the lower layer were washed with ethanol, and this was repeated 5 times. Pour the washed microspheres into a petri dish, and dry the...

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Abstract

The present invention is preparation process of micron level monodispersed copolymer microsphere. Polystyrene seed is first prepared through a dispersed polymerization process; and then secondarily swelled and polymerized together with the composite monomer of styrene (St), divinyl benzene (DVB and ethylene glycol dimethyl acrylate (EGDMA) to prepare micron level St / DVB / EGDMA copolymer microsphere. The microsphere is regular, solid, homogeneous in grain size, monodispersed and heat resistant, and has strength and toughness meeting the requirement for making ACF.

Description

technical field [0001] The invention relates to a method for preparing micron-scale monodisperse copolymerized microspheres, belonging to the field of polymer material preparation. Specifically, relate to making polystyrene (PS) seed with dispersion polymerization method, adopt seed secondary swelling and polymerization technology to make the method for micron order monodisperse copolymerization microsphere namely St / DVB / EGDMA copolymerization microsphere then, wherein St is styrene, DVB is divinylbenzene, and EGDMA is ethylene glycol dimethacrylate. technical background [0002] As a functional material, monodisperse micron-sized polymer microspheres not only penetrate into all aspects of daily life, but also have entered high-tech fields such as medical and pharmaceutical fields, biochemical fields, electronic information materials, etc. . In recent years, monodisperse micron-sized polymer microspheres have opened up a new application field in the field of electronic inf...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08C08F212/36C08F220/16C08F2/38C08F2/00
Inventor 李兴存纪克兵赵士杰周小平豆帆朱洪维
Owner YANTAI SHUODE NEW MATERIAL
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